Sulfur interference

In terrestrial vegetation, molybdenum and sulfur interfere with copper-induced deficiencies (Gupta 1979). Copper poisoning in cattle and other ruminants is governed by dietary concentrations of molybdenum and sulfate (Lewis et al. 1967 Todd 1969 Buckley and Tait 1981 Eisler 1989). Molybdenum and sulfur in mammalian diets cause a decrease in the availability of copper because of the formation of the biologically unavailable copper-thiomolybdate complex (Aaseth and Norseth 1986). Cattle die when grazing for extended periods on pastures where the ratio of copper to molybdenum... 

While all planar aromatic PLACs and RPCBBs of interest were persistent against sulfuric acid, the cleanup of the evaporated extract in hexane was started by sulfuric acid shaking or with sulfuric acid impregnated on a silica column [43,56]. For sediment samples, elemental sulfur interference was eliminated using copper activated with HC1 [43, 57]. Further cleanup of PLACs was done according to Scheme 1 [43]. 

Goerhtz, D. F. and Law, L. M., Note on removal of sulfur interferences from sediment extracts for pesticide analysis. Bull. Environ. Contam. Toxicol., 6, 9-10, 1971. 

Another view is that sulfur interferes with the antidegradant activity (in this case with IPPD) [55]. 

Both nitrogen and sulfur interfere at concentrations greater than approximately 0.1 %. 

The presence of sulfur, nitrogen, halogens, etc. can interfere with the test. After pyrolysis, it is necessary to eliminate the following components ... 

Orga.nic Carbon. Organic materials interfere with plant operation because these compounds react with sulfuric acid under furnace conditions to form sulfur dioxide. There is a reducing atmosphere in the furnace which may reduce sulfur dioxide to elemental sulfur, which results in sulfur deposits in the gas handling system. 

Electrica.1 Properties. The electrical properties of SF stem primarily from its effectiveness as an electron scavenger. To accomplish electrical breakdown in a dielectric gas, primary electrons must gain sufficient energy to generate appreciable numbers of secondary electrons on molecular impact. Sulfur hexafluoride interferes with this process by capturing the primary electrons, resulting in the formation of SF or SF ions and F atoms (29) ... 

The biochemical basis for the toxicity of mercury and mercury compounds results from its ability to form covalent bonds readily with sulfur. Prior to reaction with sulfur, however, the mercury must be metabolized to the divalent cation. When the sulfur is in the form of a sulfhydryl (— SH) group, divalent mercury replaces the hydrogen atom to form mercaptides, X—Hg— SR and Hg(SR)2, where X is an electronegative radical and R is protein (36). Sulfhydryl compounds are called mercaptans because of their ability to capture mercury. Even in low concentrations divalent mercury is capable of inactivating sulfhydryl enzymes and thus causes interference with cellular metaboHsm and function (31—34). Mercury also combines with other ligands of physiological importance such as phosphoryl, carboxyl, amide, and amine groups. It is unclear whether these latter interactions contribute to its toxicity (31,36). 

Qualitative Analysis. Nitric acid may be detected by the classical brown-ring test, the copper-turnings test, the reduction of nitrate to ammonia by active metal or alloy, or the nitrogen precipitation test. Nitrous acid or nitrites interfere with most of these tests, but such interference may be eliminated by acidifying with sulfuric acid, adding ammonium sulfate crystals, and evaporating to alow volume. 

Analytical and Test Methods. o-Nitrotoluene can be analyzed for purity and isomer content by infrared spectroscopy with an accuracy of about 1%. -Nitrotoluene content can be estimated by the decomposition of the isomeric toluene diazonium chlorides because the ortho and meta isomers decompose more readily than the para isomer. A colorimetric method for determining the content of the various isomers is based on the color which forms when the mononitrotoluenes are dissolved in sulfuric acid (45). From the absorption of the sulfuric acid solution at 436 and 305 nm, the ortho and para isomer content can be deterrnined, and the meta isomer can be obtained by difference. However, this and other colorimetric methods are subject to possible interferences from other aromatic nitro compounds. A titrimetric method, based on the reduction of the nitro group with titanium(III) sulfate or chloride, can be used to determine mononitrotoluenes (32). Chromatographic methods, eg, gas chromatography or high pressure Hquid chromatography, are well suited for the deterrnination of mononitrotoluenes as well as its individual isomers. Freezing points are used commonly as indicators of purity of the various isomers. 

The hberated iodine is measured spectrometricaHy or titrated with Standard sodium thiosulfate solution (I2 +28203 — 2 1 VS Og following acidification with sulfuric acid buffers are sometimes employed. The method requires measurement of the total gas volume used in the procedure. The presence of other oxidants, such as H2O2 and NO, can interfere with the analysis. The analysis is also technique-sensitive, since it can be affected by a number of variables, including temperature, time, pH, iodide concentration, sampling techniques, etc (140). A detailed procedure is given in Reference 141. 

A method suitable for analysis of sulfur dioxide in ambient air and sensitive to 0.003—5 ppm involves aspirating a measured air sample through a solution of potassium or sodium tetrachloromercurate, with the resultant formation of a dichlorosulfitomercurate. Ethylenediaminetetraacetic acid (EDTA) disodium salt is added to this solution to complex heavy metals which can interfere by oxidation of the sulfur dioxide. The sample is also treated with 0.6 wt % sulfamic acid to destroy any nitrite anions. Then the sample is treated with formaldehyde and specially purified acid-bleached rosaniline containing phosphoric acid to control pH. This reacts with the dichlorosulfitomercurate to form an intensely colored rosaniline—methanesulfonic acid. The pH of the solution is adjusted to 1.6 0.1 with phosphoric acid, and the absorbance is read spectrophotometricaHy at 548 nm (273). 

Although gravimetric methods have been used traditionally for the determination of large amounts of tellurium, more accurate and convenient volumetric methods are favored. The oxidation of teUurium(IV) by ceric sulfate in hot sulfuric acid solution in the presence of chromic ion as catalyst affords a convenient volumetric method for the determination of tellurium (32). Selenium(IV) does not interfere if the sulfuric acid is less than 2 N in concentration. Excess ceric sulfate is added, the excess being titrated with ferrous ammonium sulfate using o-phenanthroline ferrous—sulfate as indicator. The ceric sulfate method is best appHed in tellurium-rich materials such as refined tellurium or tellurium compounds. 

Catalytic Oxidation. Catalytic oxidation is used only for gaseous streams because combustion reactions take place on the surface of the catalyst which otherwise would be covered by soHd material. Common catalysts are palladium [7440-05-3] and platinum [7440-06-4]. Because of the catalytic boost, operating temperatures and residence times are much lower which reduce operating costs. Catalysts in any treatment system are susceptible to poisoning (masking of or interference with the active sites). Catalysts can be poisoned or deactivated by sulfur, bismuth [7440-69-9] phosphoms [7723-14-0] arsenic, antimony, mercury, lead, zinc, tin [7440-31-5] or halogens (notably chlorine) platinum catalysts can tolerate sulfur compounds, but can be poisoned by chlorine. 

Fluoride. A fluoride concentration of ca 1 mg/L is helpful in preventing dental caries. Eluoride is deterrnined potentiometrically with an ion-selective electrode. A buffer solution of high total ionic strength is added to the solution to eliminate variations in sample ionic strength and to maintain the sample at pH 5—8, the optimum range for measurement. (Cyclohexylenedinitrilo)tetraacetic acid (CDTA) is usually added to the buffer solution to complex aluminum and thereby prevent its interference. If fluoroborate ion is present, the sample should be distilled from a concentrated sulfuric acid solution to hydrolyze the fluoroborate to free fluoride prior to the electrode measurement (26,27). 

Several colorimetric procedures for fluoride are available, but it is usually desirable to distill the sample from concentrated sulfuric acid prior to analysis to eliminate interferences. One method is based upon bleaching a dye formed by the reaction of zirconium and sodium 2-(p-sulfophenylazo)-l,8-dihydroxy-3,6-naphthalenedisulfonate (SPADNS reagent) (28). 

Phosphate. Phosphoms occurs in water primarily as a result of natural weathering, municipal sewage, and agricultural mnoff The most common form in water is the phosphate ion. A sample containing phosphate can react with ammonium molybdate to form molybdophosphoric acid (H2P(Mo202q)4). This compound is reduced with stannous chloride in sulfuric acid to form a colored molybdenum-blue complex, which can be measured colorimetrically. SiUca and arsenic are the chief interferences. 

Two colorimetric methods are recommended for boron analysis. One is the curcumin method, where the sample is acidified and evaporated after addition of curcumin reagent. A red product called rosocyanine remains it is dissolved in 95 wt % ethanol and measured photometrically. Nitrate concentrations >20 mg/L interfere with this method. Another colorimetric method is based upon the reaction between boron and carminic acid in concentrated sulfuric acid to form a bluish-red or blue product. Boron concentrations can also be deterrnined by atomic absorption spectroscopy with a nitrous oxide—acetjiene flame or graphite furnace. Atomic emission with an argon plasma source can also be used for boron measurement. 

Compounds that induce bronchoconstriction include tobacco smoke, formaldehyde, and diethyl ether. Several other compounds, such as acidic fumes (e.g., sulfuric acid) and gases, such as ozone and nitrogen dioxide, as well as isocyanates, can cause bronchoconstriction. Also, cellular damage in the airways induces bronchoconstriction because of the release of vasoactive compounds. Frequently, different mechanisms work at the same time, provoking bronchoconstriction and increased secretion of mucus, both of which interfere with respiration. 

Estrone methyl ether (100 g, 0.35 mole) is mixed with 100 ml of absolute ethanol, 100 ml of benzene and 200 ml of triethyl orthoformate. Concentrated sulfuric acid (1.55 ml) is added and the mixture is stirred at room temperature for 2 hr. The mixture is then made alkaline by the addition of excess tetra-methylguanidine (ca. 4 ml) and the organic solvents are removed. The residue is dissolved in heptane and the solution is filtered through Celite to prevent emulsions in the following extraction. The solution is then washed threetimes with 500 ml of 10 % sodium hydroxide solution in methanol to remove excess triethyl orthoformate, which would interfere with the Birch reduction solvent system. The heptane solution is dried over sodium sulfate and the solvent is removed. The residue is satisfactory for the Birch reduction step. Infrared analysis shows that the material contains 1.3-1.5% of estrone methyl ether. The pure ketal may be obtained by crystallization from anhydrous ethanol, mp 99-100°. Acidification of the methanolic sodium hydroxide washes affords 10-12 g of recovered estrone methyl ether. 

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